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By Alfred V. de Forest

WE are now assembled in this hall for the eighteenth lecture in honor of the memory of our greatest American metallurgist, Henry Marion Howe. Many of his most intimate contemporaries, led, as was fitting, by Professor Sauveur, have described his vital accomplishments in three fields: as a leader in technical industrial development; in theoretical research; and finally as a teacher and source of inspiration for nearly two generations of students. In 1914 Professor Howe had retired from active teaching, but maintained his laboratory at Columbia University under the care of Arthur G. Levy, with whom he published many of the papers that later were incorporated into his last book, "The Metallography of Steel and Cast Iron." My position at the time was that of personal assistant to Professor Campbell-no pay, no duties, but the great privilege of preparing specimens, taking pictures and attending to some of the current consulting work. Whenever possible, I visited Howe's laboratory to chat with Levy and gather ideas about the wonderful field of metallography-in which I was a rank amateur, rescued by the quiet enthusiasm of Donald Smith of Princeton from an instructorship in civil engineering. Levy let me act as a fly on the wall during the Professor's occasional visits. Busy as he was, Professor Howe took the time and trouble to encourage my interest, as he had done for hundreds of others. He told me how he went about gathering his own information speculating as to causes, considering experiments, and verifying his conclusions. I ventured to mention some tests I had run on the irregular stretching of wires of different metals. He read the small volume I had prepared of ill-assorted facts and fancies and remarked: "Nobody cares for your theories or the history of your tests. Describe what you found as briefly as possible and perhaps I can help you to publish." Curiously enough, among my discards were some autographically recorded load-versus-electrical-resistance measurements. Taken with inadequate knowledge and equipment, these curves did not reproduce consistently, but if the relationship between strain and resistance had then been explored, the latest type of strain gauge might have been in useful service for the past 25 years. Professor Howe was a gifted teacher, perhaps because he was primarily an ardent and assiduous student. His own eagerness to learn and his willingness to revise and extend his opinions constantly encouraged those of his environment to be diligent and painstaking in the pursuit of knowledge. In honoring his memory, I also wish to bring to mind the kindly, humorous and quiet Levy, and join his name again, as it was for too brief a space in the past, with that of many-sided Henry Marion Howe. FACTORS OF IMPACT STRENGTH The subject chosen for the Howe Memorial Lecture by Dr. Gillett last year

Jan 1, 1941

By Alfred V. de Forest

We are now assembled in this hall for the eighteenth lecture in honor of the memory of our greatest American metallurgist, Henry Marion Howe. Many of his most intimate contemporaries, led, as was fitting, by Professor Sauveur, have described his vital accomplishments in three fields: as a leader in technical industrial development; in theoretical research; and finally as a teacher and source of inspiration for nearly two generations of students. In 1914 Professor Howe had retired from active teaching, but maintained his laboratory at Columbia University under the care of Arthur G. Levy, with whom he published many of the papers that later were incorporated into his last book, " The Metallography of Steel and Cast Iron." My position at the time was that of personal assistant to Professor Campbell—no pay, no duties, but the great privilege of preparing specimens, taking pictures and attending to some of the current consulting work. Whenever possible, I visited Howe's laboratory to chat with Levy and gather ideas about the wonderful field of metallography—in which I was a rank amateur, rescued by the quiet enthusiasm of Donald Smith of Princeton from an instructorship in civil engineering. Levy let me act as a fly on the wall during the Professor's occasional visits. Busy as he was, Professor Howe took the time and trouble to encourage my interest, as he had done for hun- dreds of others. He told me how he went about gathering his own information speculating as to causes, considering experiments, and verifying his conclusions. I ventured to mention some tests I had run on the irregular stretching of wires of different metals. He read the small volume I had prepared of ill-assorted facts and fancies and remarked: "Nobody cares for your theories or the history of your tests. Describe what you found as briefly as possible and perhaps I can help you to publish." Curiously enough, among my discards were some autographically recorded load-versus-electrical-resistance measurements. Taken with inadequate knowledge and equipment, these curves did not reproduce consistently, but if the relationship between strain and resistance had then been explored, the latest type of strain gauge might have been in useful service for the past 25 years. Professor Howe was a gifted teacher, perhaps because he was primarily an ardent and assiduous student. His own eagerness to learn and his willingness to revise and extend his opinions constantly encouraged those of his environment to be diligent and painstaking in the pursuit of knowledge. In honoring his memory, I also wish to bring to mind the kindly, humorous and quiet Levy, and join his name again, as it was for too brief a space in the past, with that of many-sided Henry Marion Howe. Factors oF Impact Strength The subject chosen for the Howe Memorial Lecture by Dr. Gillett last year

Jan 1, 1941

By Alfred V. de Forest

We are now assembled in this hall for the eighteenth lecture in honor of the memory of our greatest American metallurgist, Henry Marion Howe. Many of his most intimate contemporaries, led, as was fitting, by Professor Sauveur, have described his vital accomplishments in three fields: as a leader in technical industrial development; in theoretical research; and finally as a teacher and source of inspiration for nearly two generations of students. In 1914 Professor Howe had retired from active teaching, but maintained his laboratory at Columbia University under the care of Arthur G. Levy, with whom he published many of the papers that later were incorporated into his last book, " The Metallography of Steel and Cast Iron." My position at the time was that of personal assistant to Professor Campbell—no pay, no duties, but the great privilege of preparing specimens, taking pictures and attending to some of the current consulting work. Whenever possible, I visited Howe's laboratory to chat with Levy and gather ideas about the wonderful field of metallography—in which I was a rank amateur, rescued by the quiet enthusiasm of Donald Smith of Princeton from an instructorship in civil engineering. Levy let me act as a fly on the wall during the Professor's occasional visits. Busy as he was, Professor Howe took the time and trouble to encourage my interest, as he had done for hun- dreds of others. He told me how he went about gathering his own information speculating as to causes, considering experiments, and verifying his conclusions. I ventured to mention some tests I had run on the irregular stretching of wires of different metals. He read the small volume I had prepared of ill-assorted facts and fancies and remarked: "Nobody cares for your theories or the history of your tests. Describe what you found as briefly as possible and perhaps I can help you to publish." Curiously enough, among my discards were some autographically recorded load-versus-electrical-resistance measurements. Taken with inadequate knowledge and equipment, these curves did not reproduce consistently, but if the relationship between strain and resistance had then been explored, the latest type of strain gauge might have been in useful service for the past 25 years. Professor Howe was a gifted teacher, perhaps because he was primarily an ardent and assiduous student. His own eagerness to learn and his willingness to revise and extend his opinions constantly encouraged those of his environment to be diligent and painstaking in the pursuit of knowledge. In honoring his memory, I also wish to bring to mind the kindly, humorous and quiet Levy, and join his name again, as it was for too brief a space in the past, with that of many-sided Henry Marion Howe. Factors oF Impact Strength The subject chosen for the Howe Memorial Lecture by Dr. Gillett last year

Jan 1, 1941

By W. P. Sykes

IN CONNECTION with a study of tungsten steels, Honda and Murakami1 reported an investigation of the system iron-tungsten. This report included a tentative equilibrium diagram, photomicrographs of various alloys in the series, and qualitative measurements of hardness and magnetic properties. The present investigation originally had as its object the study of the hardness and tensile properties of a series of carbon-free iron-tungsten alloys. But, as the work progressed it became evident that the system possessed other features of interest, so the scope of the investigation was enlarged. MATERIALS The iron powder used in preparing the alloys was obtained as follows: Iron oxalate was precipitated from a ferrous-sulfate solution by the addition of a solution of oxalic acid. This oxalate, after thorough washing, was ignited to iron oxide, which after reduction in hydrogen at about 1000° C. yielded iron powder containing but about 0.2 per cent. iron oxide and about 0.005 percent. carbon. Tungsten metal in the form of powder, such as is used in the manufacture of filaments for incandescent lamps, was the other constituent. This material analyzed 99.8 per cent. tungsten and contained no carbon, The metal powders, in the desired proportions, were mixed by tumbling and formed, under pressure of 20 tons per sq. in., into rods 3/8 by 3/8 by 10 in. To form the alloys without contamination, sections of the pressed rods were placed on alundum slabs and heated in an alundum tube wound with a tungsten resistor and packed in heat-insulating material. While the resistor was heated, a stream of hydrogen was continually passed through both the tube and the case containing it. The tungsten winding on the tube, as well as the material heated within the tube, was thus protected from oxidation. Such a furnace will operate constantly

Jan 2, 1926

ECONOMICS In the preceding pages you will find an attempt to judge the direction of one phase of the mining industry in Drift, and following that a quick round up of what happened to production in 1958 in Trends. Next, Charles Merrill presents a comprehensive price history for the mineral products of greatest importance, complete with figures for the past 50 years. On the following pages Nathaniel Arbiter and Charles Will Wright take a look at price trend prospects and the cold war in mining, respectively. MINERALS BENEFICIATION Fifty years progress is reviewed as a springboard for a look ahead. In the past decade the art has moved forward, but the author fears that the science is not progressing as promisingly.

Jan 2, 1959

By E. D. Gardner

FIFTY years ago the Utah Copper enterprise at Bingham was just getting under way. An epic in metal mining was in the making. Throughout the West the bonanza deposits were approaching exhaustion and most ore still went direct to smelter. But concentrators were shortly to be constructed for treating milling grade ores, and most important, the pilot plant for the Utah Copper enterprise was being built that year at the mouth of Bingham Canyon. The same decade was to see development at the Inspiration mine in Arizona of the most important new mining method for 50 years to come—undercut block caving. Although the average grade of ore being mined has been declining for 50 years, and wage rates and prices of supplies have been greatly increased, the mining industry has continued to grow and to prosper. Technology has advanced to a point where minerals can be mined under the most severe conditions. The hardest rock can be drilled and broken and the heaviest ground handled. Large or small, an ore-body can be mined successfully, at any desired rate of production. It is possible to pump great volumes of water and to ventilate the most extensive workings; air conditioning has made practicable the mining of ore where the rock temperatures are beyond those that can be borne by man. Mining today in the U. S. is a huge earth-moving operation. In 1953 nearly 2 billion tons of material were mined for direct use or for processing. Stripping at open-cut mines totaled about 1.7 billion cu yd. Table I gives relative tonnages of the branches of the mineral industry in 1953. In addition to the solid materials moved, 350 million tons of petroleum and 340,000 tons of gas were produced in 1953. Fifteen million tons of salt and 5 million tons of liquid sulphur were pumped from wells. An appreciable amount of copper was recovered by leaching old mine workings and dumps. Total value of minerals produced in 1953 was $14.4 billion: oil and gas $7.6 billion, coal $2.6 billion, nonmetallics $2.4 billion, and metals $1.8 billion. Formidable problems face some branches of the industry today, especially pertaining to increased output tons per manshift. The time has come when these problems should be reappraised. With current wage rates, the industry no longer can afford to pay men to do manual labor. It should be recognized, also, that the miner is a skilled worker; efforts to promote the dignity of his calling and his pride of accomplishment have yielded beneficial results. Mineral deposits occur under widely varying conditions. In most instances the degree of support needed by the roof and walls is the deciding factor in selection of an underground mining method. The degree of support needed, in turn, is governed by natural physical characteristics of the ore and its enclosing rocks. Mine operators, of course, learn to judge ground by observation, and an experienced mine boss generally can anticipate what will happen following any given mining operation. A more scientific approach, however, would be advantageous in most cases. More should be known about the strength of the ore and the enclosing rocks, more about stresses set up in the ground when ore is removed, and more about the mechanics of moving ground. Better understanding would work both ways: first, favorable rock conditions could be fully utilized for more efficient mining, and second, hazards of rock falls could be minimized, loss of ore in mining reduced, and expenses caused by ground pressures and subsidence lowered. In general, mining comprises breaking the ore or rock in place, supporting the mine workings, and transporting the ore to the surface. This latter is a materials handling problem. Ventilation, of course, must be provided, and the mines must be kept free of water. Development work at some places is the most important cost item in extracting ore. Drilling and blasting remain the usual practice for breaking ore or rock from place except, of course, at block-caving mines. The drilling and blasting practice at a mine must fit the mining method. In laying out mining procedures attention is being given to

Jan 1, 1956

By J. F. Keefe, C. J. Bier, O&apos

This study was carried out with copper because it represents the simplest form of sintering, in that but one metal is involved and all reactions occur in the solid state. The present work will cover three variables affecting the sintering process; namely, briquetting pressure, sintering temperature and time in hot zone. Although strength and dimensional changes were observed, this is primarily a metal-lographic study of the sintering process in copper. The term "sintering" should be understood to mean the process by which the metal powder particles of the compact become united into one body. Material Used The copper powder used was made from reduced copper oxide, and is typical of a grade used for the mass production of parts formed of metal powders. The screen analysis of the powder was as follows: Per Cent Per Cent BY BY Particle Size "Weight Particle Size "Weight Mesh Microns /80.... 0.00 43/32.... 17.49 80/I00..... 32/20......16.68 100/140.... 0.34 20/10.... 23.14 140/200___ 15.25 10/5..... 4.64 200/230....... 5.00 5/0...... 0.75 230/325.... 16.70 — 325....62. 69 The minus 325-mesh analysis was made by using a Roller Air Analyzer.1,2 The apparent density is here defined as the weight per cubic centimeter of the loose, unpacked powder as measured with the Hall flowmeter. The value for the powder used was 2.57 grams per cubic centimeter.

Jan 1, 1945

By N. V. Hansell

l. INTRODUCTION. THE last few years have shown an increasing interest in the subject of beneficiating iron-ores -in all iron-producing countries. In the United States, this movement has been slower than in certain parts of Europe, for the obvious reason that the abundance and relative cheapness of the Lake Superior iron ores has hindered the development of enterprises for the preparation of low-grade ores. Gradually, however, conditions have changed. The world's consumption of iron is increasing enormously. Being in 1900 about 40,000,000 tons, in 1910 ii was already 60,000000; and there is no reason to doubt that for the near future the increase in iron-consumption will continue at the same rapid rate, especially with, the development of China, certain parts of Africa, and other regions which have hardly been touched as yet by modern industrialism. It is. therefore, not surprising that apprehension is felt that the known available iron-ore resources of the world are gradually being depleted. Signs of this feeling are the recent investigation, under the direction of the U. S. Geological Survey, of the iron-ore resources of the United States, and the estimate presented to the last International Geological Congress, at Stockholm, Sweden, of the iron-ore resources of the world. These investigations have emphasized the fact that the known high-grade ore-deposits are limited in extent, and will, at a not distant future, be exhausted, compelling the iron industry to depend for raw material on the enormous deposits of low-grade ores which are distributed over almost all the world. The discovery of new deposits of high-grade ore, in countries not yet thoroughly explored, will not materially change this prospect. Of course, the part which such new deposits will play in the future cannot be forecast. The difficulty and cost of transportation will probably exclude many of them from use at the present centers of the iron industry.

May 1, 1912

By Owen Thornton

Recently equations have been presented by Rose and Bruce' and by Rose², showing how the relative permeability of a reservoir rock may be determined from the capillary character of the rock. In particular, equations were developed to show the relationship between capillary pressure and the effective permeability to the wetting phase in a poly-phase flow system. The equations are as follows (nomenclature the same as in the Rose and Bruce paper) Rose and Bruce assume that the average length of path (L,), which the wetting fluid follows in flowing through a porous media is independent of the saturation to the wetting phase, so that 1 is a constant dependent only on the k rock, and the permeability to the wetting phase is a function of the saturation and of the capillnry pressure: In measuring the flow of ekctric current through partially saturated core samples, it has been observed that the electrical resistance usually is not a simple linear function of saturation. This fact indicates that the average length of path in the flow of electric current is not independent of saturation, but rather that the tortuosity of the path depends upon the average saturation to the conducting fluid as well as upon the characteristics of the rock. itself. Inasmuch as the flow of fluid and the flow of electric current in many respects are analogous, it may be indicated further that the length of path for fluid also may not be independent of saturation. The following relationship can be derived to express the resistance to flow of electric current through a core sample partially saturated with conductive wetting phase, the non-wetting phase being non-conductive: where L is the average length of path followed by the current in flowing through a length L of partially saturated core, where L is the length of current path when the core is fully saturated, and where Rs and R, are the specific resistivities of the partially saturated and saturated core sample, respectively. It will be noted that R., the specific resistivity of the core sample when S, = 1.0, is equal to the "formation resistivity factor"' multiplied by the specific resistivity of the saturating fluid. If it be assumed that the average lengths of path for fluid flow and for the flow of electric current are the same, then equation (5) may be combined with equations (l), (2) and (3) to give the following relationship: The above equation suggests including a correction for tortuosity when calculating the relative permeability of a reservoir rock to a wetting phase. The correction factor may be obtained from the resistivity-saturation relationship. For instance, the following calcu- lations are obtained for the unconsoli-dated sands described by Leverett Kw Kw Sw R°/Rs Pt/Pc¹ (Calc.) (Obs.) 0.30 0.08 0.88 0.02 0.0 0.40 0.16 0.94 0.06 0.04 0.50 0.27 0.97 0.14 0.11 0.60 0.40 0.98 0.26 0.21 0.70 0.53 0.98 0.39 0.35 0.80 0.68 0.99 0.57 0.54 0.90 0.84 0.99 0.77 0.76 1.00 1.00 1.00 1.00 1.00 It will be noted that the agreement between the calculated points and the observed data is rather good. Further investigation of the above method for obtaining relative permeabilities may be merited. For many sands within specified ranges of saturations the following relationship has been found to hold approximately': — =SW"......(7) Rs The exponent n in the above equation has been found to equal two for many sands so that equation (6) reduces to the following: The writer acknowledges the permission of The Texas Co. to submit this note for publication. 1. Walter Rose and W. A. Bruce—Jnl. of Pet. Tech., Vol. 1, No. 5, p. 127 (1949). 2. Walter Rose—Jnl. of Petr. Tech., Vol. 1, No. 5, p. 111 (1949). 3. G. E. Archie— -Trans. AIME, 146, 54 (1942). 4. M. C. Leverett— Trans. AIME, 142, 152 (1941). 5. M. C. Leverett—Trans. AIME, 132, 149 (1939).

Jan 1, 1949

By Owen Thornton

Recently equations have been presented by Rose and Bruce' and by Rose², showing how the relative permeability of a reservoir rock may be determined from the capillary character of the rock. In particular, equations were developed to show the relationship between capillary pressure and the effective permeability to the wetting phase in a poly-phase flow system. The equations are as follows (nomenclature the same as in the Rose and Bruce paper) Rose and Bruce assume that the average length of path (L,), which the wetting fluid follows in flowing through a porous media is independent of the saturation to the wetting phase, so that 1 is a constant dependent only on the k rock, and the permeability to the wetting phase is a function of the saturation and of the capillnry pressure: In measuring the flow of ekctric current through partially saturated core samples, it has been observed that the electrical resistance usually is not a simple linear function of saturation. This fact indicates that the average length of path in the flow of electric current is not independent of saturation, but rather that the tortuosity of the path depends upon the average saturation to the conducting fluid as well as upon the characteristics of the rock. itself. Inasmuch as the flow of fluid and the flow of electric current in many respects are analogous, it may be indicated further that the length of path for fluid also may not be independent of saturation. The following relationship can be derived to express the resistance to flow of electric current through a core sample partially saturated with conductive wetting phase, the non-wetting phase being non-conductive: where L is the average length of path followed by the current in flowing through a length L of partially saturated core, where L is the length of current path when the core is fully saturated, and where Rs and R, are the specific resistivities of the partially saturated and saturated core sample, respectively. It will be noted that R., the specific resistivity of the core sample when S, = 1.0, is equal to the "formation resistivity factor"' multiplied by the specific resistivity of the saturating fluid. If it be assumed that the average lengths of path for fluid flow and for the flow of electric current are the same, then equation (5) may be combined with equations (l), (2) and (3) to give the following relationship: The above equation suggests including a correction for tortuosity when calculating the relative permeability of a reservoir rock to a wetting phase. The correction factor may be obtained from the resistivity-saturation relationship. For instance, the following calcu- lations are obtained for the unconsoli-dated sands described by Leverett Kw Kw Sw R°/Rs Pt/Pc¹ (Calc.) (Obs.) 0.30 0.08 0.88 0.02 0.0 0.40 0.16 0.94 0.06 0.04 0.50 0.27 0.97 0.14 0.11 0.60 0.40 0.98 0.26 0.21 0.70 0.53 0.98 0.39 0.35 0.80 0.68 0.99 0.57 0.54 0.90 0.84 0.99 0.77 0.76 1.00 1.00 1.00 1.00 1.00 It will be noted that the agreement between the calculated points and the observed data is rather good. Further investigation of the above method for obtaining relative permeabilities may be merited. For many sands within specified ranges of saturations the following relationship has been found to hold approximately': — =SW"......(7) Rs The exponent n in the above equation has been found to equal two for many sands so that equation (6) reduces to the following: The writer acknowledges the permission of The Texas Co. to submit this note for publication. 1. Walter Rose and W. A. Bruce—Jnl. of Pet. Tech., Vol. 1, No. 5, p. 127 (1949). 2. Walter Rose—Jnl. of Petr. Tech., Vol. 1, No. 5, p. 111 (1949). 3. G. E. Archie— -Trans. AIME, 146, 54 (1942). 4. M. C. Leverett— Trans. AIME, 142, 152 (1941). 5. M. C. Leverett—Trans. AIME, 132, 149 (1939).

Jan 1, 1949

By A. T. Aldred

HIS note reports the existence of several new scandium intermetallic compounds of the A2B and AB stoichiometries where the A element is scandium and the B element is from group VIII or IB of the periodic table. Alloys were arc melted from high-purity materials using 2-g charges. Typical lot analyses for the materials used are given in Table I. Chemical analyses were not made on the alloys as there was little or no weight loss on melting. After annealing the specimens for 14 days at 600°C and water quenching, metallographic and X-ray techniques were used to determine the occurrence of the various phases. Table II lists the relevant data for the A2B phases. The Ti2Ni structure,2 has ninety-six atoms in a face-centered cubic cell, whilst the Al2Cu structure is body-centered tetragonal.3 The occurrence and stability of the various A2B type phases in transition metal alloy systems has recently been considered by Nevitt.4 The Ti2 Ni-type phases occur over a relatively narrow range of radius ratios from 1.14-1.26 with A partners mainly from the titanium group and B partners predominantly from the cobalt group. This suggests that both a favorable relative size of the atoms and a favorable electron concentration are necessary conditions for the existence of this structure type. A12Cu-type phases involving Ti group elements as A partners are formed with B partners from the cobalt and nickel groups, predominantly the latter, and have a higher radius ratio (1.27-1.29) than the Ti2Ni-type phases. The occurrence of both Sc2Pd and Sc2Co can be rationalized in terms of these considerations but SczNi is anomalous because of its high radius ratio. The radius ratios are calculated from the Goldschmidt CN12 radii and it might be postulated that the scandium atom is reduced in size in the compound. Unfortunately the apparent atomic size of scandium in the compound cannot be calculated from a knowledge of the structure and lattice dimensions. The crystal structure of the Sc2Au compound could not be identified from the powder diffraction pattern, but it is interesting to note that it is isostructural with a series of A2Au phases where A is a rare earth element.5 Pertinent information concerning the AB phases found in this investigation is given in Table 111. All the phases have the ordered bcc CsCl structure. The occurrence and stability of CsC1-type phases have recently been discussed by Dwight,7 who concludes that the relative sizes of the atoms do not appear to be a controlling factor (the radius ratios of all the known phases vary between 0.985 and 1.439) but that the occurrence of the phase is predominantly dependent on the relative positions of the A and B partners in the periodic table. As a measure of the stability of a given CsCl phase it has been customary to define a lattice contraction on alloying, DAB — dAB, where DAB is the AB interatomic spacing as calculated from the Goldschmidt CN8 radii and dAB is the AB interatomic distance in the compound (= v3/2 ao). Values of the parameter DscB -dScB for the compounds found in this investigation are given in column 5 of Table III and are plotted in Fig. 1. If the lattice contraction does in fact reflect the stability of a phase then Fig. 1 shows two very interesting trends when the position of the B partner in the periodic table is considered. Firstly, within any given group the stability increases in order on going from the first to third long period. Secondly, within any given period the stability increases in order as the B partner is taken from the copper, nickel, and cobalt groups. In the case of the second long period, the lattice contraction reaches a maximum at ScRh and then decreases to ScRu. The same trend could

Jan 1, 1962

By H. N. Treaftis, J. W. Cahn

THE previous determinations of the solvus of tin in solid lead disagree with one another by as much as 40°C or almost 10 at. pct. Even determinations that appear to be careful differ considerably in both the solubility and its temperature coefficient. Recent kinetic workl -3 on the rate of precipitation of tin from lead-tin alloys and thermodynamic work4 on the heat of solution of tin in lead have given some insight into the time necessary to reach equilibrium in this system. As this time is longer than that used in almost all previous determinations of the solvus, these determinations are questionable. Since the interpretation of recent kinetic results requires accurate values of the equilibrium solubility the present work was undertaken. DISCUSSION OF PREVIOUS RESULTS The methods used in previous studies may be placed into three classes: 1) Several alloys covering a range of compositions are allowed to reach "equilibrium" at a certain temperature.5-7 Some property, such as the X-ray lattice parameter of the lead-rich phase or the re- sistivity of the alloy, is then measured as a function of composition. The solubility limit for that temperature is taken to be that composition at which a discontinuity in the property occurs. However, the recent kinetic work has shown that tin precipitates in two stages. The first stage is rapid but leaves the lead still supersaturated. The second stage is very slow, and it seems from the equilibration times quoted by the investigators of the solvus that the end of the first stage of precipitation was usually mistaken for equilibrium. This is especially true at temperatures below 100°C where the first reaction is still quite rapid (from minutes to months), but where the second stage is so slow that very long holding times are required to reach equilibrium. Alternatively micrographic work8 on several alloys of different compositions seems to have given good results if done carefully. 2) The beginning of precipitation in a homogenized alloy is measured as it cools slowly8-10. Since reactions in solids undercool easily, such determinations will always give too low a temperature for the solvus. 3) Some property of an alloy is measured as a function of temperature while the alloy is above the solvus.5,9,11 The range of temperature can usually be extended slightly into the two phase region. Then the alloy is precipitated at a much lower temperature and slowly reheated. The solvus is taken to be the lowest temperature where the property of the reheated alloy is equal to that previously determined for the homogeneous alloy. Usually one also expects a discontinuity at the solvus in the temperature variation of the property for the reheated alloy. The difficulty in this method is the sluggishness of the dissolution process, and this method may give too high a solvus temperature. EXPERIMENTAL The phase boundary or solvus temperature was determined by a modification of method 3 for a series of chemically analyzed high-purity alloys, ranging from 5.1 to 26.4 at. pct Sn. The resistance, as a function of temperature, of a sample of homogenized alloy (which could easily be undercooled) was compared with the equilibrium resistance which that alloy sample attained after precipitation at room temperature followed by long isothermal anneals at various temperatures. Before each anneal the sample was rehomogenized and reprecipitated. The solvus temperature could be located to within 1°C as the intersection of the resistance vs temperature curves for the homogenized and equilibrium alloys. No attempt was made to locate the phase boundary more accurately since the limiting factor was the precision with which the alloys could be analyzed. This precision was ±0.1 wt pct Sn and corresponds to an error of 1 deg in temperature. This use of isothermal anneals differs from some of the previous investigations in which method 3 was used with baths of slowly rising temperatures. It was found early in the investigation that solvus temperatures tended to be high if the latter method was used even at extremely slow heating rates. For example a

Jan 1, 1961

By L. W. Rowe, S. S. Cole

A laboratory bench scale unit is described whereby finely divided chlorinatable residues are held for a short period by a restraining bed of a coarse-grained ore of comparable composition to permit 'flash' chlorination of the high surface area powder. Results on chlorinating a finely divicled titania residue using rutile sand as the restraining bed showed that 92 pct utilization of chlorine and equivalent conversion of TiO2 in the fine residue to Ticl4 were attained with a dust loss of about 3 to 4 pct and an equivalent amount of ch1om'nation of the titanium values in the restraining bed. THE chlorination of coarse grain titaniferous ores; i.e., 20 to 150 mesh sizes in fluidized beds is practiced commercially.' One effective method found for the chlorination of a very fine material in a fluidized bed is the "flash" chlorination technique.' By charging the finely divided charge material into the bottom of an established bed of optimum sized rutile, ilmenite, titanium beneficiate, or even an inert material such as sand, chlorination occurs before the dust can pass through the bed. The major requirement is that the bed be less chlorinatable than the charge. In this process, the charge consists of a finely divided (between one and 50 µ) titania residue obtained from a titaniferous ore beneficiation process. The charge is blended with a 20 pct wt basis addition of 20 to 60 .mesh size low volatile coke (to minimize hydrogen chloride formation) and fed to the bottom of the bed with the chlorine gas stream. A ball check device is used to permit entry of the charge and prevent the bed from discharging when the gas flow is cut off. The coarse pieces of coke serve to reduce compaction in the charge mixture and permit sat]sfactory feeding without plugging or jamming. Feed and gas rates are adjusted to provide for complete reaction of the charge material, with 90 to 95 pct chlorine efficiency, and maintain a gas flow in the range of 0.4 to 0.6 ft per sec. The equipment consisted of a 3-in. diam mullite tube enclosed in an electric furnace. A bow-shaped 3/4 in. Saran tube fed the charge from an air lock type of feed hopper (to prevent the escape of the chlorine gas into feed bin) to the bottom of the bed. The charge rate was set by providing a small awiliary hopper below the feed hopper where a weighed portion of the charge could be discharged in a specified time interval into the main chlorine stream. The chlorine rate was measured by a flowmeter. The reaction tube was filled with a bed of Australian rutile ore, this restraining bed serving two purposes; i.e., it rapidly heated the fresh charge to the reaction temperature and retained the particles in the bed for a sufficient time for selective chlorination to proceed. Due to the fine particle size and open, porous structure of the charge, this reaction was almost instantaneous, and, with proper adjustment of feed and gas rates, very little fine material passed through the bed without reacting and only a very small fraction of the restraining bed was chlorinated. A typical reaction procedure was to fill the bench scale fluidized bed unit with a 1 kg charge of Australian rutile ore analyzing 95.5 pct TiO2, 0.6 pct FeO, a beach sand deposit 40 to 150 mesh size. When fluidized, the bed was approximately 2 ft in depth. The ore was fluidized with a 1:l mixture of chlorine and nitrogen at a rate of 0.40 ft per sec. This gas mixture was necessitated by the comparatively short bed depth; a larger unit, with a deeper bed, could be fluidized with chlorine alone without significant free chlorine loss. Feed rate was 8.0 g per min of beneficiated ilmenite analyzing 85.0 pct TiO2, 2.6 pct FeO plus 1.6 g per min of 20 to 60 mesh petroleum coke. The

Jan 1, 1962

By John D. Price

R. W. Campbell (Jones and Laughlin Steel Carp., Pittsburgh)—As usual John Price has presented an excellent paper. I know of no one who has devoted more time and conscientious thought to this subject than he has, and his efforts have produced scientific data and conclusions of real value. Results of similar studies made by the Jones and Laughlin Steel Corp. on the blending of Pennsylvania coals may be of interest. During 1935 the late F. W. Wagner and the present writer developed an empirical physical fuel value formula for evaluating the combined physical tests of metallurgical coke, see Table IV. In the development of the formula, the tumbler test, shatter test, screen test, and porosity of coke have been taken into consideration. Each of these tests brings out some physical property not expressed by the others, and in estimation of the importance of these tests as a medium for evaluating coke for the blast furnace, their worth has been graded as follows: It was thought that some additional penalty should be applied to cokes that do not show a uniform screen size, assuming that coke larger than 4 in. was not desirable and that this size was an indication of irregular size. Therefore the screen test factor is further corrected by applying a penalty of 1 pct for each 1 pct material greater than 4-in. size as shown by the screen test. The physical fitness of coke for blast furnace use depends upon four fundamental characteristics: l—gen-era1 strength, as indicated by the shatter test; 2— abradability, or the resistance of cell walls to reduction in size by attrition, as indicated by the tumbler test; 3—porosity; and 4—size and uniformity. Each of these characteristics is not of equal importance, but surely, in an attempt to determine an accurate physical value, the individual value of each should be taken into consideration. The formula is used as a yardstick, so to speak, in determining variations in the normal production of metallurgical coke and in making comparisons between normal coke and experimental blends with other coals. Table IV gives results of coking tests on raw and washed high volatile coals and these same coals with blends of coke breeze, anthracite coal, char and low volatile coals, all from Pennsylvania. The table also gives the source of the coals and coke breeze, as well as their proximate analyses. It will be noted that the washing of the raw high volatile coal increased the physical fuel value from 26.17 to 39.16, showing the effect of removing shale and slate which produces a detrimental fracturing and weakening of the coke. It is a well known fact that many Pennsylvania high volatile coals contain an excess of resinous material or binder which has a tendency to weaken the coke, owing to its high evolution of gases during carbonization. Tests were therefore made with coke breeze, an inert material, in an attempt to alleviate this condition. Blends of washed coal with 5 pct and 7.5 pct coke breeze collected from the coke plant quenching sump (82.9 pct through 1/8-in. screen) resulted in cokes with a physical fuel value of 20.75 and 16.73 respectively, lower than results obtained from 100 pct raw high volatile coal. It will be noted that the percentage of + 4-in. coke increased but that the tumbler test was very low. Undoubtedly better results could have been obtained if the coke breeze could have been crushed extremely fine. During World War II the government asked the coking industry to consider the use of anthracite coal as a substitute for high quality low volatile coal, which was extremely scarce at the time. The next series of tests was made with blends of raw and washed high volatile coals and 5, 10, and 15 pct Pennsylvania No. 5 buckwheat anthracite (100 pct through l/8-in. screen). It was necessary to use some raw high volatile coal in these blends because of insufficient washer capacity at the time. It will be noted that the physical fuel values

Jan 1, 1954

Edward Dyer Peters, the only child of Henry Hunter Peters and Susan Barker Thaxter, was born in Dorchester, Mass., June 1, 1849. From his father he was a descendant of the Peters family of Ipswich and Andover, Mass., whose earliest ancestor settled in Essex County in 1659; while upon his mother's side he descended from several old Hingham families, as well as from the Quineys and from Governor Bradford. Between the ages of fourteen and sixteen he was a student at the Episcopal School for boys in Cheshire, Conn. Near the school was an old tin mine, and he used to spend his Saturday afternoons exploring it. When Edward was sixteen, his father sold his property in South-borough, and for the next three years lived in Europe. Sept. 26, 1865, Edward entered the Royal School of Mines at Freiberg, Saxony. In the summer of 1867 he joined his family on Lake Geneva, and spent a part of the season in that vicinity, going to Chamounix and taking other trips. Extract from a letter to his father: Elbingerode, Harz, Aug. 30, 1868: I left Freiberg with my friend Lilienthal, on Wednesday the 19th of August, reached Leipzig in the evening and spent the night in that city: the next morning we took the cars and in the afternoon reached Eisleben, in Prussia, which was to be our first stopping-place; there are immense copper-mines and smelting-works at this place, and the method of working the mines is very peculiar ... The next morning we got up at five and spent the whole day in the smelting-works where I obtained a number of drawings of the furnaces they use here and a good many valuable data. Saturday morning we got up at four o'clock, and descended a mine about three miles from the town; the Director of this mine was one of the most intelligent and agreeable men that I ever met; he accompanied us in the mine and explained everything that was new to us. The system of mining at Eisleben is peculiar to this town, and is not used at any other place in the world; the copper ore comes in narrow, flat veins eighteen inches high, at the utmost, consequently the men work lying flat on their left side and using the pick with both hands: the ore is carried out of the side passages into the main ones, in very low waggons about twelve inches high, and four by two feet; the boys who pull these waggons have a board buckled to their left thigh and their left arm; they pass their bare foot through a strap in the waggon and wriggle along on their side dragging the waggon after them, with their foot, almost as fast as a man can walk above ground. In the afternoon we walked over to Hittstadt, about twelve miles, and remained there Sunday and Monday. Monday night, at ten o'clock we went out to one of the smelting-works, to see the refining of the copper; this is only done at night, so we worked there from ten in the evening till eleven the next morning, and came home all blackened up and with blistered hands, for our skin was not quite so tough as that of the workmen: at noon the same day we took the stage to Ascherls-leben, and then the train to Stassfurt, where there are immense salt-mines, as well as factories for the manufacture of bromium, which latter process is, however, kept a profound secret, so we had very little hope of seeing anything but the salt mines; we were talking with our landlord about our disappointment, that evening, when he told us that the director of the Bromium works was sitting in the next room with no company but his glass of beer, so we went over to him, introduced ourselves as Americans, and actually succeeded in persuading him that it could do his business no earthly hurt if he showed us his works; at last he consented, after making us give our word of honor

Jan 1, 1919

By R. M. S. B. Horta, W. T. Roberts, D. V. Wilson

Evaluation of results obtained by the Harris method for inverse pole figures is discussed. Two existing analyses and a new approach are compared. In the most frequently used analysis, different reflections are accorded equal weight. A second method involves area-weighting of reflections, mainly to take account of nonuniformity of Pole distribution. In the new method, reflections are weighted according to their multiplicity factors. Intensity ratios obtained from a sample of steel sheet by the three methods are compared. INVERSE pole figures offer a convenient method of depicting the proportions of material with various orientations referred to a unique specimen axis. The technique was first applied to fiber textures, but it is now frequently used as a description of texture in sheet metal, the unique axis in this case usually being the sheet normal. The Harris method' for the determination of inverse pole figures has the great merit of simplicity. It suffers certain intrinsic limitations, but provided that these are borne in mind, the results allow useful conclusions to be drawn regarding the effects of texture components on certain mechanical properties. Much thought has been given to alternative methods of texture description, aimed at eliminating the ambiguity in the simpler methods.2"6 Refinements in the method of description are obtained at the price of increasing complexity, and it seems clear that a simple method, such as that of Harris, will continue to find application. The original derivation by Harris1 has been corrected by Morris7 and later by Mueller, Chernock, and Beck.2 Since the latter reference is more accessible, it is referred to more frequently than the work of Morris. Most users of the inverse pole figure method present their results on the basis of the treatment by Mueller et al., and it is the purpose of the present communication to comment on this treatment and to suggest a simple modification to the method of presentation which enhances the meaningfulness of the results. It will be convenient first to summarize the Mueller analysis as follows: The intensity Ihkl of a hkl reflection from a textured specimen is: Ihkl=CI0AL\Fhkl\2NhklPhkl [1] where C is a constant for a given sample I, is the intensity of the incident beam A is an absorption factor. With usual diffrac-tometer geometry and a flat specimen, A is inversely proportional to the density of the specimen. L is the Lorenz polarization factor Fhkl is the structure factor for the hkl reflection Nhkl is the multiplicity factor phkl is the fraction of crystals in the polycrystal-line aggregate with any particular (nkl) plane parallel to the surface. The corresponding equation for a specimen with randomly oriented grains is lR,hkl=CRl°ARL\fnkl\2Nnklk [2] the subscripts R indicating the factors that are different for the random sample, which will, in general, have a density different from that of the textured one. The intensity ratio is hkl , c A Phkl [3] IR,hkl CR AR PR The constants are eliminated by summing over all the measured reflections ^iRMi °R AR PR ljPkkl and from Eqs. [3] and [4] T IR,hkl The only unknown in Eq. [5] is Yj phkl and before this can be evaluated, it is necessary to adopt some form of normalizing procedure. Mueller et al. assume that when a large number, n, of reflections is used, the average value of p as defined by Eq. [6] below will be unity ? = £j**l3l [6] and the final result of their analysis follows: hkl Pkkl = i I&Jf~ [7] ±y* Ihkl ^ in,hki The normalizing procedure used by Mueller et al. involves an unrealistic assumption since it gives equal weight to each of the hkl reflections. Other normalizing procedures can now be examined with a view to selecting a more appropriate one. For an infinite number of reflections, the function p can be averaged over a continuous range of orientations covering the complete solid angle 4p by the integral relation: p =1 jp(a)dQ = l [8] This is the only exact procedure, but in practice a

Jan 1, 1970

By B. Yarar, J. Kaoma

[Introduction The critical surface tension of wetting of hydrophobic materials has been investigated extensively by Zisman et al. (1973) and relates the spreading of a liquid on a solid to the surface tension of this liquid. Thus, the Zisman ap¬proach shows that a plot of Cos 0 versus ?LV where, 0 is the contact angle and ?LV is the surface tension of that liquid in contact with its own vapor at equilibrium, produces a straight line which can be extrapolated to Cos 0 = 1. The intercept corresponds to a given ?LV, termed the critical surface tension of wetting. In instances, however, Cos 0 - ?LV plots show deviations from linearity. Alternative approaches have also included the plotting of adhesion tension (YLV COs 0) versus ?LV that can be interpreted in terms of critical surface tension data (Lucassen-Reynders, 1963). It has, on the other hand, been customary to correlate contact angle (0) with flotation data, although it is recognized that surface inhomogeneities and related contact angle hysteresis limit the interpretations pertaining to solid surface structures purely based on contact angle measurements. It is nonetheless true that 0 = 0, when the liquid is water, corresponds to a hydrophilic solid. Determination of ?c by contact angle measurements in conformity with the Zisman approach can encounter experimental difficulties, especially when solids are in a powder form. Following the reasoning that 0 = 0 corresponds to the hydrophilic state of a solid, froth flotation experiments can be expected to produce critical surface tension of wetting values for powders. The technique that consists of plotting recovery (% R) versus YLV data and extrapolating the linear part of the curve to % R = 0, has been described elsewhere (Yarar and Kaoma, 1984). This paper describes some of the results obtained by the extrapolation technique mentioned above, using various sulfide minerals. Experimental Materials Molybdenite (MoS2), sphalerite (ZnS), chalcopyrite (CuFeS2), chalcocite (Cu2S), and galena (PbS) were handsorted from massive samples and ground by mortar and pestle, and the -147 Fan fraction used in experiments; sulfur (S) was a C.P. Fisher Scientific Co. product. Method One gram powder samples were conditioned for three minutes in methanol-water solutions of predetermined surface tension values and the percents recovered by flotation using a Partridge-Smith Cell (Partridge and Smith, 1972), were plotted against each ?LV value. Results and Discussion The percent recovery versus ?LV for two naturally hydrophobic solids, i.e., natural molybdenite, MoS2 and sulfur are given in Fig. 1 where it is seen that ?c for sulfur is obtained as 31.5 mNm-1 whereas for MoS2, it is 26 mNm-1. Figure 1 also shows that the new flotation technique described, for estimating ?c is in good agreement with the Zisman method. Curves obtained by the same method for the minerals Cu2S, PbS, and ZnS are given in Fig. 2, where it is seen that for Cu2S, ZnS, and PbS, the extrapolation to % R = 0 produces ?c values of 36, 39, and 49 mNm-1, respectively. CuFeS2, on the other hand, gives a curve that does not permit such an extrapolation to obtain a ?c value with certainty. Nonetheless, treatment of the powder with 8.95 X 10-5 molar Na2S solution followed by washing with distilled water prior to flotation effects the curves as shown in the insert of Fig. 2. The type of curves given in Fig. 1 appear to be typical of hydrophobic solids as can also be observed in Fig. 3. The composition of solid and minute quantities of inclusions seem to play an important role as regards the surface properties of solids as reflected by the slope of the linear part of the % R - ?LV plot and thus the value of ?c obtained by this technique. For example, MoS2 of three different stoichiometric compositions produced the data given below. [MoS2MoS2.14Mo1.002S2 ?c mNm-126.029.031.0 dR/d?8.95.23.0]]

Jan 1, 1985

By Antoni Kidybinski

Mechanical properties of the nether roof rocks play a substantial role in maintenance of mine openings. On longwall faces too low strength is a cause of rock- falls which bring about delays in face advance, and hazard to the miners, while too high strength may result in over hanging of roof rocks in gobs, sometimes over a large area, initiating dynamic periodical pressures. Hence, efforts have been undertaken to develop methods of caveability evaluation for proper selection of roof control system and of longwall-face supports. DESCRIPTIVE CLASSIFICATIONS One of the basic qualitative criteria for classification of roof types with different caveability is the criterion of geological structure. The 26-stages scale worked out for conditions of Donetz Coalfield. USSR, by E.T. Proyavkin et al.(l) may be an example of that type of classification. This scale is presented graphically in Fig. 1. The first types of roofs according to this scale are easily caving immediately after exposure of a small surface, while the last be- long to the strongest roofs which over-hang in waste and require artificial fracturing. Observations and measurements carried out also in Donetz mines lead W.T. Davidyanc (2) to following classification: Class I - weak and densely bedded rocks very easily caving after each advance of supports. The roof subsidence over a waste edge is: [ ] where: h is roof subsidence, m M is thickness of the seam being mined, m S is width of an opening, m Class II - medium caveability and small main roof movements [ ] Class III - hardly breakable rocks, thicker beds with higher strength: caving by large blocks. After exposure of larger roof surfaces the movements of the main roof strata may affect an opening. [ ] Class IV - very hardly breakable rocks - thick, monolithic sandstones: they cause considerable difficulties in working with caving. [ ] Class V - thin-bedded rocks featured by the capacity of a smooth subsidence without disintegration into loose blocks with keeping contact between the particular blocks in a bed. In this classification mining with full roof caving is recommended for class I-III and only exceptionally for class IV. In many coal fields, qualitative and quantitative observations of roof rocks behavior have been carried out: as a result relations and characteristics found in certain mines are given. As an example, Kizielov Coalfield data in the USSR given by B.S. Vinokur (3) may be mentioned. In working thin pitching seams man- less system of undercutting the seam by means of rope saw is used there. The author separated four classes of roofs and gave, for every class, the empirical relation between the extracted area and the time of roof stability. The size of the stable area of exposed roof for particular classes is as follows: 120 to 150 m2 (1291 to 1614 ft2 ), 170 to 200 m2 (1829 to 2152 ft2), 250 to 280 m2 (2690 to 3013 ft2 ) and 350 to 400 m2 (3766 to 4300 ft ). For Kuznetz coalfield in the USSR the following classification of roofs was developed at the WIMI Institute in Leningrad: Class I - completely unstable: impact strength in- dex of rock f = up to 1.5 - the strip of roof 1.4 to 2.0 m (4.59 to 6.56 it) wide, exposed after shearer's cut holds stable during the time not longer than 5 min. Class II - low stability: f = 1.5 to 2.5 - the strip of roof 1.4 to 2.0 m (4.59 to 6.56 ft) wide and up to 4.0 m (13 it) long, exposed after shearer's cut holds stable during 5 to 20 min. Class III - medium stability: f = 2.51 to 3.5 - the strip of roof 1.4 to 2.0 m (4.59 to 6.56 it) wide and 4.0 to 25 m (13 to 82 ft) long, exposed after shearer's cut holds stable from 20 min. to 2 hours. Class IV - stable: f = 3.51 to 4.5 - the strip of roof 1.4 to 2.0 m (4.59 to 6.56 ft) wide and 25 m (82 it) long exposed after shearer's cut is stable during the time longer than 2 hours. Class V - entirely stable: f = over 4.5

Jan 1, 1982

By A. H. Daane, B. J. Beaudry

The Sc-Y and Sc-Zr systems were studied by thermal and X-ray methods. Both systems are characterized by complete solid solubility in the low temperature hexagonal form and in the high temperature bcc form. In the Sc-Y system, there is a minimum in the solidus at 50 at. pct and 1365°C, while the solidus in the Sc-Zr system follows a nearly straight line relationship between the melting point of scandium and zirconium. There is a minimum in the temperature of transition from hexagonal to bcc in the Sc-Y system at 43 at. pct Y and 1175°C; while the temperature of transition is raised in the Sc-Zr system to a maximum of 1415 °C at 30 at. pct Zr. INTEREST in the metals of the first transition series has usually stemmed from their useful properties; however, there is now a great deal of interest in determining the fundamental nature of these metals. Since scandium is the first of these transition metals, a study of the preparation and Properties1 and the alloying behavior of scandium2 was initiated. In a continuing study of the alloying behavior of scandium, the systems of scandium with zirconium and yttrium have been established. Extensive solid solubility in both the Sc-Zr and Sc-Y systems was expected from application of the classical rules of Hume-Rothery. Also, the modified Darken and Gurry plot as suggested by Gschneid-ner3 showed ideal conditions for solubility in the Sc-Zr system with less favorable conditions in the Sc-Y system. The effect of scandium on the transformation temperature of zirconium and yttrium was of interest, since a recent empirical observation by Uly and Burr4 predicted that the solute scandium would raise the transformation temperature of zirconium and lower the yttrium transformation. In addition to noting the validity of the above predictions, the SC-Y and Sc-Zr systems were established. EXPERIMENTAL METHODS Materials. The metals employed in this investigation were crystal bar zirconium, distilled scandium prepared by the method described by Spedding, et al.1 and yttrium prepared by the method described by Carlson, et a1.5 The major impurities present in these metals are listed in Table I in ppm. Alloy Preparation. All the alloys examined were initially formed by comelting the two metals in a nonconsumable electrode arc-melting furnace under an atmosphere of purified helium or argon. The buttons were inverted at least five times and re-melted each time to ensure homogeneity. During preparation of Sc-Zr alloys, approximately 1 wt pct was lost which was attributed entirely to the loss of scandium by distillation. When preparing Sc-Y alloys, approximately 1.5 wt pct was lost, but it was assumed that the intended composition was maintained, since the relative weight lost when arc melting the component metals was nearly the same. Samples weighing 15 to 20 g were prepared for time-temperature thermal analysis, while only 1- to 2-g samples were prepared for the optical pyrometer and X-ray diffraction studies. Thermal Methods. The solidus and the melting points of the metals were determined by an optical pyrometer method described previously.2 The temperatures at which the transformation from hexagonal to bcc occurs were determined by differential thermal analysis. Several points on the solidus and liquidus in the Sc-Y system were also determined by this method and are in good agreement with those obtained by the optical pyrometer method. The procedure followed in the preparation of samples for thermal analysis and the furnace used have been described elsewhere.2'6 Since a limited quantity of scandium was available, most of the alloys were not melted during thermal analysis, thus avoiding contamination by the crucible. The alloy could then be reused and the composition changed by adding the desired quantity of solute to obtain the next alloy. Heat Treatment and X-Ray Methods. In order to ensure homogeneity, the "as arc-melted" alloys Were wrapped in tantalum foil, sealed in quartz capsules and heated at 1100°C for 15 hr and then cooled at a rate of 8 deg per min. Samples for X-ray diffraction were filed from these heat-treated alloys, sealed in 1/8 in. by 1/2 in. tantalum capsules under

Jan 1, 1963

By R. F. Mehl, C. E. Birchenall

SINCE Maxwell1 first considered the self-diffusion process in 1872 its importance in the kinetic theory of matter has been recognized. Until the discovery of isotopes in 1913, a direct measurement of this quantity seemed impossible. The only information that could be gathered indirectly was for gaseous systems for which the kinetic theory was well developed. When methods of direct observation be-came available, investigations on self-diffusion were carried out in condensed phases. In metals these data are presumably of potential importance in the study of recovery, recrystallization, creep, sintering, and related phenomena. Following the pioneer work of Von Hevesy2 and his collaborators, who determined the rate of self-diffusion in lead with the naturally occurring thorium B isotope, several metals have been investigated. Pb, Ag³, Au.6,5, and Cu6,7,8,9 are examples of isotropic crystals existing in only one phase modification. Anisotropy of diffusion has been demonstrated in Bil6 and Znll. This paper is a study of a single metal in two allotropic forms and also of self-diffusion in a body-centered cubic lattice. Despite the fact that the measurements in each of the papers cited on self-diffusion in copper seem to be internally consistent to about 10 to 15 pet, the curves reported by different authors differ by factors of 2 to 4 at the same temperatures. This uncertainty may account, in part, for the failure to establish a successful correlation between the self-diffusion rates and other physical characteristics of the metals. No satisfactory theory of metallic self- diffusion has as yet been proposed to account for all the existing data and to permit estimation in other metals. Experimental Part: Two units of radioactive iron were used in these experiments, each a mixture of Fe53 and Fe59 (12). Fe53 decays by K electron capture and the emission of an X ray with a half life of about 4 years. Fe59 emits two beta spectra, one with a maximum energy of 0.26 Mev, the other 0.46 Mev, and gamma rays of 1.1 and 1.3 Mev, with a half life of about 44 days. They were present in nearly equal concentration initially. The composite half life started at about 50 days and increased as the Fe59 decayed, leaving Fe55 relatively more abundant. After aging a year, the half life was too long to measure significant decay in a month. The absorption properties also changed with time. Because of the importance of the absorption coefficient in the diffusion calculations, it was necessary to determine this quantity frequently over the period during which these experiments were carried out. This correction was unsuspected at the time of publication of notesl3 on this work and accounts for the discrepancy in alpha iron and for part of the discrepancy in gamma iron.* * The data in the present paper supersede those given in the notes entirely. In one note the scale of log D was inadvertently reversed. In addition to the correction for the drift in absorption coefficient, the D values for gamma iron at low temperatures were high owing to insuficient correction for diffusion occurring during heating and cooling through the high temperature part of the alpha range at a rate much slower than that employed in the runs reported here. The high temperature alpha rates are much higher than the low temperature gamma rates and correspond to large equivalent times at these temperatures. These experiments were discarded and new measurements taken. Independent experiments with the same activity units indicated a radioactive contaminant in the iron, but exhaustive attempts to isolate and identify it chemically failed. These experiments? indicate † These experiments will be discussed in a later publication from this laboratory. that the contaminant represented only a trace of little importance in the diffusion results. The active iron was plated from an iron chloride solution. Enough of the solution was dropped on a 1% in. square of filter paper to wet it thoroughly.

Jan 1, 1951